OBJECTIVE： To establish a method for simultaneous determination of BHT， free sulfur， antioxidant 1010， antioxidant 330， antioxidant 1076 and antioxidant 168 in pharmaceutical halogenated butyl rubber stopper. METHODS： HPLC method was adopted. The determination was performed on Agilent Zorbax SB-C18 column with mobile phase consisted of methanol-water （gradient elution） at the flow rate of 1.0 mL/min. The column temperature was 25 ℃， and detection wavelength was set at 220 nm. The sample size was 10 μL. RESULTS： The linear ranges of BHT， free sulfur， antioxidant 1010， antioxidant 330， antioxidant 1076 and antioxidant 168 were 2.592-64.80 μg/mL （r＝0.999 9）， 2.648-66.20 μg/mL （r＝0.999 9）， 2.062-51.55 μg/mL （r＝0.999 9）， 2.654-66.35 μg/mL （r＝0.999 9）， 2.128-53.20 μg/mL （r＝0.999 9）， 2.468-61.70 μg/mL （r＝0.999 9）， respectively. The limits of quantitation were 2.073 6， 2.118 4， 2.749 2， 1.061 6， 4.436 0， 3.090 4 mg/kg； the limits of detection were 0.628 4， 0.641 9， 0.833 1， 0.321 7， 1.344 2， 0.992 4 mg/kg， respectively. RSDs of precision， stability and reproducibility tests were all lower than 3％. The average recoveries were 96.57％-99.17％（RSD＝0.92％， n＝9）， 77.47％-86.14％（RSD＝2.94％， n＝9）， 96.11％-98.39％（RSD＝0.63％， n＝9）， 96.22％-98.33％（RSD＝0.67％， n＝9）， 95.59％-99.22％（RSD＝1.11％， n＝9） and 81.54％-88.31％（RSD＝2.46％， n＝9）， respectively. CONCLUSIONS： The method is sensitive， rapid， convenient and reproducible， and can be used for simultaneous determination of 5 antioxidant and free sulfur in pharmaceutical halogenated butyl rubber stopper.